Fly ash is one of the aluminosilicate sources used for the synthesis of geopolymers. The particle size distribution of fly ash and the content of unburned carbon residue are known to affect the compressive strength of geopolymers. In this study, the effects of particle size and unburned carbon content of fly ash on the compressive strength of geopolymers have been studied over a compositional range in geopolymer gels. Unburned carbon was effectively separated in the -46μm fraction using an air classifier and the fixed carbon content declined from 3.04 wt% to 0.06 wt%. The mean particle size (d50) decreased from 22.17μm to 10.79μm. Size separation of fly ash by air classification resulted in reduced particle size and carbon residue content with a collateral increase in reactivity with alkali activators. Geopolymers produced from carbon-free ash, which was separated by air classification, developed up to 50 % higher compressive strength compared to geopolymers synthesized from raw ash. It was presumed that porous carbon particles hinder geopolymerization by trapping vitreous spheres in the pores of carbon particles and allowing them to remain intact in spite of alkaline attack. The microstructure of the geopolymers did not vary considerably with compressive strength, but the highest connectivity of the geopolymer gel network was achieved when the Si/Al ratio of the geopolymer gel was 5.0.